CN101466858B - 具有细化结构的硬质合金 - Google Patents

具有细化结构的硬质合金 Download PDF

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CN101466858B
CN101466858B CN2007800221360A CN200780022136A CN101466858B CN 101466858 B CN101466858 B CN 101466858B CN 2007800221360 A CN2007800221360 A CN 2007800221360A CN 200780022136 A CN200780022136 A CN 200780022136A CN 101466858 B CN101466858 B CN 101466858B
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莱夫·阿克松
苏珊·诺格伦
亚历山大·库索夫斯基
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Abstract

本发明涉及一种WC-Co硬质合金。通过加入极少量的Ti、V、Zr、Ta或Nb，或者它们的组合，得到一种含有较少异常WC晶粒的晶粒细化硬质合金结构。

Description

具有细化结构的硬质合金
本发明涉及一种硬质合金。通过加入极少量的Ti、V、Zr、Ta或Nb，或上述这些的组合，已经得到了一种具有较少异常WC晶粒的晶粒细化的硬质合金。
硬质合金切削工具被用于对韧度和耐磨性均有较高要求的对钢、淬火钢、不锈钢、铸铁和耐热合金的加工中。为了达到所期望的性质，除WC和Co之外，通常需要加入像TiC、NbC、TaC、ZrC和HfC的立方碳化物。这些立方碳化物将在微观结构中形成第三相，立方面心碳化物(B1)，通常被称作γ相。无论是细小晶粒还是正常晶粒的硬质合金，在烧结期间都必须控制晶粒生长。众所周知，当在没有抑制剂的情况下烧结WC-Co等级时，WC晶粒的生长非常快，并会发生异常晶粒生长，以至在结构中出现非常大的WC晶粒。因为这些异常晶粒作为严重缺陷并会导致破坏，所以可能对于切削操作是有害的。一种公知控制晶粒生长的方法是添加前述立方碳化物，通常碳化物为TiC、NbC、TaC、ZrC、HfC。然而，这些添加物通常为这样的量，即：使得立方碳化物相存在于微观结构中。但是，缺点是与标准的WC-Co等级相比，韧性降低。
另一种控制晶粒生长的方法是EP-A-1500713中描述的在氮气中烧结，该文献公开了一种细小晶粒的碳化钨-钴硬质合金的制造方法，该方法包括以下步骤：混合，根据标准操作研磨，随后烧结。在脱腊之后，但在孔关闭之前，通过将大于0.5个大气压的氮气引入烧结气氛中，能够得到包括降低的晶粒尺寸和较少量的异常晶粒的晶粒细化结构。
WO 2006/043421公开了一种硬质合金，其包括平均粒径＜0.3μm的WC，作为硬质相，以及5.5～15wt％的至少一种铁族金属元素，作为粘结相，除了上述硬质相和粘结相之外，还包含0.005～0.06wt％的Ti，Cr，相对于粘结相重量比率为0.04～0.2。特别地，上述硬质合金不含Ta。上述硬质合金由WC组成，所述WC在合金中形成均匀细小的颗粒，并有效地抑制了粗大WC的生长，这使得提供给硬质合金优良的强度和韧度。
本发明的目的是避免和减少现有技术的问题。
本发明的再一个目的是提供一种硬质合金切削工具，其具有改善的粘结相分布和减少的异常WC晶粒数量，给出的硬质合金工具具有改善的机械和切削性能。
现在令人惊奇地发现，通过将ppm水平的Ti、V、Nb、Zr或Ta，或它们的组合引入硬质合金中，能够得到明显的晶粒细化效果以及改善的粘结相分布。
图1是根据现有技术硬质合金微观结构的光学显微照片。
图2是根据本发明硬质合金微观结构的光学显微照片。
该硬质合金体包含晶粒尺寸为1.0～2.5μm的碳化钨，3～15wt％的钴，以及另外还有ppm水平的下述另外的元素：Ti、V、Nb、Zr、Ta或它们的混合物，使得比例
Me/Co＝(at％Ti+at％V+at％Nb+at％Zr+at％Ta)/at％Co  (at％＝原子％)
低于或等于0.014-(CW)*0.008并高于0.0005，优选高于0.0007，CW为0.80～0.95，优选为0.83～0.92，其中
CW＝磁性％Co/wt％Co
其中磁性％Co是硬质合金中磁性钴的重量百分比，wt％Co是硬质合金中钴的重量百分比。CW是Co粘结相中钨的含量的函数。CW为约1表示在粘结相中的钨含量非常低，CW为0.75～0.8表示在粘结相中的钨含量较高。
烧结体中还可以包含少量＜0.5％的另外的相(如eta相)的析出，或立方MX碳化物或碳氮化物，其中M＝(V+Zr+Ti+Ta+Nb+W)，X＝C或N。
第一优选实施方式中，另外的元素是Ti。
第二优选实施方式中，另外的元素是Ti和Ta的混合物。
第三优选实施方式中，另外的元素是Ti、Ta和Nb的混合物。
第四优选实施方式中，另外的元素是Ti和Zr的混合物。
第五优选实施方式中，硬质合金包含0.01～0.10wt％的N。
第六优选实施方式中，另外的元素是Ti或者Ti和Ta的混合物，这两种情况中，N都大于0.02wt％，优选大于0.03wt％而小于0.10wt％的N。
根据本发明的制造硬质合金的方法包括以下步骤：根据标准操作对WC-Co体进行混合、研磨、压制和烧结。加入ppm水平的Ti、V、Nb、Zr或Ta或它们的混合物，加入的量使得在烧结的硬质合金中满足根据上述的Me/Co值和CW值。Ti、V、Nb、Zr或Ta可以以纯金属的形式添加，或以碳化物、氮化物和/或碳氮化物或它们的混合物的形式添加。
实施例1
制备除了WC和9.25wt％的Co外具有下列组分(wt％)的硬质合金体1A～1F。
表1a(元素wt％，以碳化物加入)
  变体   Ti   V   Zr   Ta   Nb
  1A   --   --   --   --   --   参照
  1B   0.025   --   --   --   --   本发明
  1C   --   0.027   --   --   --   本发明
  1D   0.02   --   0.025   --   --   本发明
  1E   --   --   --   0.095   --   本发明
  1F   --   --   --   --   0.049   本发明
将所述混合物分别湿磨、烘干、压实，并在40毫巴压力下，氩保护气氛中于1410℃下烧结1小时。烧结之后，确定CW、Me/Co、0.014-(CW)*0.008值以及烧结后的晶粒尺寸，结果显示在表1b中。
表1b
  变体   CW   Me/Co   0.014-(CW)*0.008   烧结后dwc(μm)
  1A   0.91   NA   NA   1.7
  1B   0.90   0.00331   0.00680   1.4
  1C   0.89   0.00331   0.00688   1.3
  1D   0.91   0.00441   0.00672   1.4
  1E   0.91   0.00331   0.00672   1.3
  1F   0.90   0.00331   0.00680   1.4
NA＝不适用
表中清楚的表明添加少量立方碳化物样品对烧结的WC晶粒尺寸具有令人惊讶的效果。
实施例2
按照与实施例1相同的方法制备具有表2a中给出组分的硬质合金变体2A～2E。采用得自H.C.Starck公司的WC粉末和含有0.08wt％的氮的碳化钨粉末，它们均具有粒度为1.3μm的FSSS晶粒尺寸，将上述粉末连同得自OMG公司的细晶粒钴粉末和得自H.C.Starck公司的细晶粒TiC、TaC以及NbC一起使用。
表2a元素wt％
  元素wt％ Co Ti Ta Nb N WC
  2A   6.0   -   -   -   -   余量   参照
  2B   6.0   0.030   -   -   -   余量   本发明
  2C   6.0   0.010   0.009   -   0.06   余量   本发明
  2D   6.0   0.007   0.009   0.007   0.06   余量   本发明
  2E   6.0   -   0.014   0.014   0.06   余量   本发明
所述混合物分别经由湿磨、烘干、压紧，并在40毫巴压力下，氩保护气氛中于1450℃下烧结1小时。烧结完成后，确定CW、Me/Co、0.014-(CW)*0.008以及烧结后的晶粒尺寸，结果显示在表2b中。
另外，所述烧结体还要经过切削、磨削、抛光和蚀刻。通过光学显微镜观察研究其横截面并计算出在任一方向上的大于10μm的碳化钨晶粒的数量。结果显示在表2b中。
表2b
CW Me/Co 0.014-0.008*CW   dwc(μm)   ＞10μm的WC晶粒数量/cm2
  2A   0.90   NA   NA   1.8   133   参照图1
  2B   0.90   0.00616   0.00680   1.4   19   本发明图2
  2C   0.88   0.00257   0.00696   1.5   21   本发明
  2D   0.90   0.00267   0.00680   1.5   24   本发明
  2E   0.88   0.00387   0.00696   1.6   35   本发明
通过实施例1和2可以明显得出，由于少量Ti、Ta、Zr、Nb或V添加物的强的晶粒细化效果，根据本发明的变体具有的微观结构有少得多的大晶粒和普遍更细化的晶粒尺寸。

Claims (8)

1.一种WC-Co硬质合金，其特征在于WC晶粒尺寸为1.0～2.5μm，Co含量为3～15wt％，以及另外还有ppm水平的下列元素：Ti、V、Nb、Zr或Ta，或它们的混合物，使得比例
Me/Co＝(at％Ti+at％V+at％Nb+at％Zr+at％Ta)/at％Co，
其低于或等于0.014-(CW)*0.008并高于0.0005，CW为0.80～0.95，其中
CW＝磁性％Co/wt％Co
其中磁性％Co为磁性钴的重量百分比，并且wt％Co为硬质合金中钴的重量百分比。
2.根据权利要求1所述的硬质合金，其特征在于另外的元素是Ti。
3.根据权利要求1所述的硬质合金，其特征在于另外的元素是Ti和Ta的混合物。
4.根据权利要求1所述的硬质合金，其特征在于另外的元素是Ti、Ta和Nb的混合物。
5.根据权利要求1所述的硬质合金，其特征在于另外的元素是Ti和Zr的混合物。
6.根据前述任一权利要求所述的硬质合金，其特征在于其包含0.01～0.10wt％的N。
7.根据权利要求1所述的硬质合金，其特征在于另外的元素是Ti或者Ti和Ta的混合物，在这两种情况中，N含量都大于0.02wt％。
8.一种制造WC-Co硬质合金的方法，包括以下步骤：混合和湿磨WC和Co的粉末，压制以及烧结，其特征在于将ppm水平的Ti、V、Nb、Zr或Ta，或它们的混合物，以纯金属形式或者以碳化物、氮化物和/或碳氮化物形式或它们的混合物形式，以这样的量加入粉末混合物中，即：使得
Me/Co＝(at％Ti+at％V+at％Nb+at％Zr+at％Ta)/at％Co
低于或等于0.014-(CW)*0.008并高于0.0005，CW为0.80～0.95，其中
CW＝磁性％Co/wt％Co
其中磁性％Co为磁性钴的重量百分比，wt％Co为硬质合金中钴的重量百分比。
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